KR20020065843A - Highly efficient fluorescent material - Google Patents
Highly efficient fluorescent material Download PDFInfo
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- KR20020065843A KR20020065843A KR1020020005392A KR20020005392A KR20020065843A KR 20020065843 A KR20020065843 A KR 20020065843A KR 1020020005392 A KR1020020005392 A KR 1020020005392A KR 20020005392 A KR20020005392 A KR 20020005392A KR 20020065843 A KR20020065843 A KR 20020065843A
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- 239000000463 material Substances 0.000 title claims abstract description 30
- 239000000126 substance Substances 0.000 claims abstract description 17
- -1 silicide nitride Chemical class 0.000 claims abstract description 16
- 229910021332 silicide Inorganic materials 0.000 claims abstract description 15
- 150000001768 cations Chemical class 0.000 claims abstract 3
- 230000005855 radiation Effects 0.000 claims description 15
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- 229910004122 SrSi Inorganic materials 0.000 claims description 2
- 239000012190 activator Substances 0.000 claims description 2
- 230000003595 spectral effect Effects 0.000 claims 3
- 230000003287 optical effect Effects 0.000 claims 1
- 229910052788 barium Inorganic materials 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 239000011575 calcium Substances 0.000 description 4
- 238000000295 emission spectrum Methods 0.000 description 4
- 239000000049 pigment Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 229940125898 compound 5 Drugs 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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Abstract
Description
본 발명은 청구범위 제 1항의 전제부에 따른 실리사이드 니트라이드의 류(class)의 형광 물질에 관한 것이다. 더욱 상세히는, 본 발명은 황색 영역에서 형광을 발하는 실리사이드 나이트라이드이다.The present invention relates to fluorescent materials of the class of silicide nitrides according to the preamble of claim 1. More specifically, the present invention is a silicide nitride which fluoresces in the yellow region.
Sr2Si5N8과 Ba2Si5N8과 같은 실리사이드 나이트라이드의 형광 물질은 Schlieper, Millus, Schlick에 의한 "Nitridosilicate II, Hochtemperatursynthesen and Kristallstrukturen von Sr2Si5N8und Ba2Si5N8"[실리사이드 나이트라이드 II, Sr2Si5N8과 Ba2Si5N8의 고온 합성과 결정 구조] (Z. anorg. allg.Chem. 621, (1995), page 1380) 논문으로부터 이미 알려져 있다. 그러나, 이 경우에는 가시 스펙트럼의 특정 영역에서 효과적인 방사를 제안할 어느 활성제도 특정되어 있지 않다.Fluorescent materials of silicide nitrides such as Sr 2 Si 5 N 8 and Ba 2 Si 5 N 8 are described by Schlieper, Millus, Schlick, "Nitridosilicate II, Hochtemperatursynthesen and Kristallstrukturen von Sr 2 Si 5 N 8 und Ba 2 Si 5 N 8 [[High Temperature Synthesis and Crystal Structure of Silicide Nitride II, Sr 2 Si 5 N 8 and Ba 2 Si 5 N 8 ] (Z. anorg. Allg. Chem. 621, (1995), page 1380). . In this case, however, no activator is specified which would suggest effective radiation in a particular region of the visible spectrum.
본 발명의 목적은 청구범위 제 1항의 전제부에 따른 형광 물질을 제공하는 것이고, 상기 형광 물질은 효율이 가능한 높으며 370에서 430 nm의 영역의 자외선 방사에 의해 효과적으로 유도될 수 있다.It is an object of the present invention to provide a fluorescent material according to the preamble of claim 1, which is as efficient as possible and can be effectively induced by ultraviolet radiation in the region of 370 to 430 nm.
본 발명의 목적은 청구항 제 1항의 특징부에 의해 달성된다. 특히 유리한 세부사항은 종속항에서 발견된다.The object of the invention is achieved by the features of claim 1. Particularly advantageous details are found in the dependent claims.
도 1은 제 1 실리사이드 나이트라이드의 방출 스펙트럼을 보여준다.1 shows the emission spectrum of the first silicide nitride.
도 2는 제 1 실리사이드 나이트라이드의 반사 스펙트럼을 보여준다.2 shows the reflection spectrum of the first silicide nitride.
도 3은 제 2 실리사이드 나이트라이드의 방출 스펙트럼을 보여준다.3 shows the emission spectrum of the second silicide nitride.
도 4는 제 2 실리사이드 나이트라이드의 반사 스펙트럼을 보여준다.4 shows the reflection spectrum of the second silicide nitride.
도 5는 백색 광원으로서 사용되는 반도체 부품을 보여준다.5 shows a semiconductor component used as a white light source.
도 6은 세 가지 형광 물질의 혼합물의 방출 스펙트럼을 보여준다.6 shows the emission spectrum of a mixture of three fluorescent materials.
이제까지는 400 nm 근방의 영역에서 효과적으로 유도될 수 있는 황색을 방출하는 고효율의 형광 물질이 없었다. 주지된, 일반적으로 사용되는 형광 물질 YAG:Ce는 370 nm 이하와 430 nm 이상의 영역에서 효과적으로 유도되지만, 400 nm 근방의 영역에서는 잘 유도되지 않는다. 그외에 셀륨이 첨가된 석류석(Ce-doped garnets)도 문제의 사용 영역에서는 미미하게 유도될 뿐이다. 따라서 완전히 다른 시스템을 개발하는 것이 필요하였다.Until now, there has been no high-efficiency fluorescent material emitting yellow that can be effectively induced in the region near 400 nm. The commonly used fluorescent substance YAG: Ce is effectively induced in the region below 370 nm and the region above 430 nm, but is not well induced in the region near 400 nm. In addition, Ce-doped garnets are only minimally induced in the area of concern. Therefore, it was necessary to develop a completely different system.
본 발명에 따르면 형광 물질의 조성은 그것이 3가의 셀륨(Ce)으로 활성화된 스트론튬(Sr) 실리사이드 나이트라이드를 구성하도록 선택된다. 이전에 알려지지않은 형광 물질 Sr2Si5N8:Ce3+은 근자외선, 특히 370내지 430 nm의 영역에서 효과적으로 흡수하고 효율적인 황색 발광을 한다. 그것은 바람직하게는 (Sr에 대해) 1에서 10 mol% Ce에 의해 활성화된다. 이 경우에 Sr은 부분적으로 (유리하게 기껏해야 30 mol%까지) Ba(바륨)및/또는 Ca(칼슘)으로 대체될 수 있다. 또다른 실시예는 SrSi7N10:Ce3+타입의 실리사이드 나이트라이드로 구성된다. 이 경우에도 역시 Sr은 Ba 및/또는 Ca에 의해 대체될 수 있다.According to the invention the composition of the fluorescent material is chosen such that it constitutes strontium (Sr) silicide nitride activated with trivalent cerium (Ce). The previously unknown fluorescent substance Sr 2 Si 5 N 8 : Ce 3+ effectively absorbs near-ultraviolet light, especially in the region of 370 to 430 nm and gives efficient yellow light emission. It is preferably activated by 1 to 10 mol% Ce (relative to Sr). In this case Sr can be partially replaced by Ba (barium) and / or Ca (calcium) (advantageously up to 30 mol%). Another embodiment consists of a silicide nitride of SrSi 7 N 10 : Ce 3+ type. In this case too, Sr can be replaced by Ba and / or Ca.
본 형광 물질은, 예를 들어 UV LED, 그렇지 않으면 램프와 같은 1차적인 UV 방사원에 의한 유도을 위한 황색 성분으로서 특히 적당하다. 따라서 WO 98/39807에서 똑같이 설명된대로 백색 또는 황색영역에서 방출하는 광원을 구현하는 것이 가능하다. 황색을 발하는 광원은 근본적으로 그 방사가 본 발명에 따른 형광 물질에 의해 완전히 황색광으로 변환되는 UV 방사를 발하는 LED에 기초한다.The present fluorescent material is particularly suitable as a yellow component for induction by primary UV radiation sources such as UV LEDs, otherwise lamps. It is therefore possible to implement a light source emitting in the white or yellow region as described equally in WO 98/39807. The yellow light source is essentially based on an LED which emits UV radiation whose radiation is completely converted to yellow light by the fluorescent material according to the invention.
특히, 이 형광 물질은 UV-LED(예를 들어 InGaN 타입)와 함께 사용될 수 있고 , UV-LED는 청색과 황색에서 방출하는 형광 물질에 의해 백색광을 생성한다. 청색 성분을 위한 후보는 본질적으로는, 예를 들어 BAM으로 알려진 BaMgAl10O17Eu2+또는 Ba5SiO4(Cl,Br)6Eu2+또는 CaLA2S4Ce3+그렇지 않으면 SCAP로 알려진 (Sr,Ba,Ca)5(PO4)3Cl:Eu2+가 공지되어 있다. 뿐만 아니라, 적색 형광 물질이 이 시스템의 색을 개선하기 위해 사용될 수 있다. (Y,La,Gd,Lu)2O2S:Eu3+, SrS:Eu2+, 그렇지 않으면 Sr2Si5N8:Eu2+(아직 공개되지 않았지만, EP-A 99 123 747.0을 참조)가 특히 적당하다.In particular, this fluorescent material can be used with a UV-LED (eg InGaN type), which produces white light by the fluorescent material emitting in blue and yellow. Candidates for the blue component are essentially BaMgAl 10 O 17 Eu 2+ or Ba 5 SiO 4 (Cl, Br) 6 Eu 2+ or CaLA 2 S 4 Ce 3+ otherwise known as BAM or otherwise known as SCAP (Sr, Ba, Ca) 5 (PO 4 ) 3 Cl: Eu 2+ is known. In addition, red fluorescent materials can be used to improve the color of this system. (Y, La, Gd, Lu) 2 O 2 S: Eu 3+ , SrS: Eu 2+ , otherwise Sr 2 Si 5 N 8 : Eu 2+ (not yet published, see EP-A 99 123 747.0 Is particularly suitable.
이하에서는, 두 개의 전형적인 실시예를 참조하여 본 발명을 좀더 상세하게 설명하고자 한다.Hereinafter, the present invention will be described in more detail with reference to two exemplary embodiments.
본 발명에 따른 형광 물질의 구체적인 예는 도 1에 나타내고, 그것은 형광물질, Ce 비율이 Sr에 의해 점유된 격자 위치의 4 mol%에 달하는 Sr2Si5N8:Ce3+의 방출에 관한 것이다. 방출의 최대치는 545 nm 에서 나타나고 평균 파장은 572 nm 이다. 색의 로커스는 x=0.395 이고 y=0.514 이다. 유도는 400 nm 에서 수행된다.A specific example of the fluorescent material according to the invention is shown in FIG. 1, which relates to the emission of Sr 2 Si 5 N 8 : Ce 3+ with a phosphor, Ce ratio of up to 4 mol% of the lattice position occupied by Sr. . The maximum emission is shown at 545 nm and the average wavelength is 572 nm. The locus of the color is x = 0.395 and y = 0.514. Induction is performed at 400 nm.
제조는 통상적인 방법으로 수행되며, 실험 재료 Sr3N2, Si3N4및 CeO2가 서로 혼합되고, 뒤이어 혼합물이 1400℃, 질소(N2)와 수소(H2)하에서 환원되는 방식으로 5시간에 걸쳐 용광로에서 베이킹된다.The preparation is carried out in a conventional manner, in which the experimental materials Sr 3 N 2 , Si 3 N 4 and CeO 2 are mixed with each other, and then the mixture is reduced under 1400 ° C., nitrogen (N 2 ) and hydrogen (H 2 ). Baked in the furnace over 5 hours.
도 2는 이 형광 물질의 확산 반사 스펙트럼을 나타낸다. 그것은 370내지 440 nm 영역에서 뚜렷한 최소치를 보여주고, 그것에 의해 이 영역에서 유도되는 뛰어난 능력을 보여준다.2 shows the diffuse reflection spectrum of this fluorescent substance. It shows a distinct minimum in the 370-440 nm region and thereby shows an excellent ability to be derived in this region.
본 발명에 따른 형광 물질의 두번째 예는 도 3에서 보여지고, 도 3은 Ce 비율이 Sr에 의해 점유된 격자 위치의 8 mol% 에 달하는 형광 물질 Sr2Si5N8:Ce3+에 관한 것이다. 방출 최대치는 554 nm에서 및 평균 파장은 579 nm이다. 색의 로커스는 x=0.414 이며 y=0.514 이다.A second example of the fluorescent material according to the invention is shown in FIG. 3, which relates to the fluorescent material Sr 2 Si 5 N 8 : Ce 3+ whose Ce ratio reaches 8 mol% of the lattice position occupied by Sr. . The emission maximum is at 554 nm and the average wavelength is 579 nm. The color locus is x = 0.414 and y = 0.514.
제조는 상술한 방법으로 수행되고, 상기 혼합물은 1400℃, 질소(N2)하에서 환원되는 방식으로 6시간에 걸쳐 오븐에서 베이킹된다.The preparation is carried out in the manner described above, and the mixture is baked in an oven over 6 hours in a manner that is reduced under 1400 ° C., nitrogen (N 2 ).
도 4는 형광 물질의 확산 반사 스펙트럼을 보여준다. 그것은 370내지 440 nm 영역에서 뚜렷한 최소치를 보여주고, 따라서 이 영역에서 유도되는 뛰어난 능력을 보여준다.4 shows the diffuse reflection spectrum of the fluorescent material. It shows distinct minimums in the 370-440 nm region, thus showing excellent ability to be derived in this region.
백색 광원의 디자인은 도 5에서 명확하게 보여준다. 광원은, 예를 들어 390 nm의 피크 방출 파장을 갖는 InGaN 타입의 칩(1)이 있는 반도체 부품이고 칩(1)은 컷아웃(cut-out)(9) 영역의 불투명한 기본 하우징(housing)(8)에 내장된다. 칩(1)은 본딩 와이어(bond wire)(14)을 통하여 제 1 단자(3)에 연결되고, 직접적으로 제 2 전기 단자(2)에 연결된다. 컷아웃(9)은 주요 구성요소로서 에폭시 주조 수지(80내지 90%의 중량) 와 형광 안료(6)(15%이하의 중량)를 포함하는 포팅 화합물(5)로 채워진다. 제 1 형광 물질은 제 1 전형적인 실시예로 보여진 실리사이드 나이트라이드인 반면, 제 2 형광 물질은 청색 영역에서 발하는 형광 물질, 여기서는 특히 Ba5SiO4(Cl,Br)6:Eu2+이다. 컷아웃은 칩(1) 또는 안료(6)의 1차 및 2차 방사의 반사체로 사용되는 벽(17)을 갖는다. 청색과 황색의 2차적인 방사의 조합은 백색을 생성하기 위해 혼합된다.The design of the white light source is clearly shown in FIG. 5. The light source is, for example, a semiconductor component with an InGaN type chip 1 having a peak emission wavelength of 390 nm and the chip 1 is an opaque base housing in the cut-out 9 region. It is built in (8). The chip 1 is connected to the first terminal 3 via a bonding wire 14 and directly to the second electrical terminal 2. The cutout 9 is filled with potting compound 5 comprising epoxy casting resin (80 to 90% by weight) and fluorescent pigment 6 (weight less than 15%) as main components. The first fluorescent material is the silicide nitride shown in the first exemplary embodiment, while the second fluorescent material is a fluorescent material emitting in the blue region, here in particular Ba 5 SiO 4 (Cl, Br) 6 : Eu 2+ . The cutout has a wall 17 which is used as a reflector of the primary and secondary radiation of the chip 1 or the pigment 6. The combination of secondary emission of blue and yellow is mixed to produce white.
또다른 전형적인 실시예에서 세 가지 형광 물질의 혼합은 형광 안료로서 사용된다. 제 1 형광 물질(i)은 제 1 실시예로서 보여진 황색 방출 실리사이드 나이트라이드 Sr2Si5N8:Ce3+이고, 제 2 형광 물질(ii)은 앞서 언급된 SCAP의 청색 방출 형광 물질이며, 제 3 형광 물질(iii)은 Sr2Si5N8:Eu2+타입의 적색 방출 형광 물질이다. 도 6은 375 nm에서 1차적인 방출을 갖는 LED의 방출 스펙트럼을 나타내며, 높은 질의 백색 감각을 전하는 전반적인 스펙트럼(G)을 형성하기 위해, 개개의 황색(i), 청색(ii), 적색(iii) 성분이 더해진다. 조합된 색의 로커스는 x=0.333, y=0.331이다. 세 가지 성분의 사용은 특히 좋은 색의 연출을 보증한다.In another exemplary embodiment a mixture of three fluorescent materials is used as fluorescent pigment. The first fluorescent substance (i) is the yellow emitting silicide nitride Sr 2 Si 5 N 8 : Ce 3+ shown as the first embodiment, the second fluorescent substance (ii) is the blue emitting fluorescent substance of the aforementioned SCAP, The third fluorescent substance (iii) is a red emitting fluorescent substance of Sr 2 Si 5 N 8 : Eu 2+ type. FIG. 6 shows the emission spectrum of an LED with primary emission at 375 nm, with individual yellow (i), blue (ii) and red (iii) to form an overall spectrum (G) that conveys a high quality white sense. ) Components are added. The locus of the combined colors is x = 0.333, y = 0.331. The use of three ingredients ensures particularly good color reproduction.
본 발명에 따른 형광 물질은 370내지 430 nm 영역에서 효과적으로 황색 방출하는 고효율 형광 물질이다. 이는 청색, 적색 방출 형광 물질과 함께 사용되어 높은 질의 백색을 방출한다.The fluorescent material according to the present invention is a highly efficient fluorescent material that emits yellow effectively in the region of 370 to 430 nm. It is used with blue and red emitting fluorescent materials to emit high quality white.
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